characterization of corn/sugar palm fiber …

CHARACTERIZATION OF CORN/SUGAR PALM FIBER-REINFORCED

CORN STARCH BIOPOLYMER HYBRID COMPOSITES

MOHAMED IBRAHIM J IBRAHIM

FK 2020 46

i

CHARACTERIZATION OF CORN/SUGAR PALM FIBER-REINFORCED

CORN STARCH BIOPOLYMER HYBRID COMPOSITES

By


Thesis Submitted to the School of Graduate Studies, Universiti Putra Malaysia,

in Fulfilment of the Requirements for the Degree of Doctor of Philosophy

December 2019

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COPYRIGHT

All material contained within the thesis, including without limitation text, logos, icons,

photographs, and all other artwork, is copyright material of Universiti Putra Malaysia

unless otherwise stated. Use may be made of any material contained within the thesis

for non-commercial purposes from the copyright holder. Commercial use of material

may only be made with the express, prior, written permission of Universiti Putra

Malaysia.

Copyright © Universiti Putra Malaysia

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Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfillment

of the requirement for the degree of Doctor of Philosophy

CHARACTERIZATION OF CORN/SUGAR PALM FIBER-REINFORCED CORN STARCH BIOPOLYMER HYBRID COMPOSITES

By


December 2019

Chairman

Faculty

: Professor Ir. Mohd Sapuan bin Salit, PhD, PEng

: Engineering

Contemporary environmental concerns, such as non-biodegradable disposal materials

and the growing mountain of garbage as well as the plant waste accumulation, are

increasingly recognized as ecological threats. Space for landfills is limited, and

additional incineration capacities require high capital investment and cause further

environmental problems. All these issues forced the researchers and scientists to move

toward manufacturing and developing eco-friendly engineering materials from

renewable sources to replace conventional non-biodegradable materials in several

applications that could preserve the green environment. Amongst these sources are

corn plant and sugar palm tree, which are a vital source for many biomasses.

Therefore, a series of lab experiments through a solution casting technique was carried

out to prepare and characterize starch, fibers, polymers, composites, and hybrid

composites in four correlated stages to achieve a hybrid composite from corn/sugar

palm fiber reinforced cornstarch.

The first stage was designed to study the chemical composition, physical properties,

thermal stability, and surface morphology of thermoplastic corn starch and corn hull,

husk, and stalk fibers, which were extracted from different corn plant parts. The

obtained samples were characterized on a powder basis. The corn husk and corn starch

revealed an excellent combination of properties. Cornhusk provided the highest

cellulose content (45.7%) as well as the most favorable surface morphology. Corn

starch revealed acceptable amylose content (24.6 g/100g) and tolerable thermal

stability with an onset melting point of 161.2 ºC. Since the cellulose and starch

demonstrated an excellent correlation between the function and structure of

biomolecules. Hence, both corn starch and husk have the potential for use in many

applications of the biomaterial.

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The second stage was accomplished to determine the effect of various concentrations

of selected plasticizers in cornstarch-based films, to prepare a new biopolymer. The

physical, morphological, thermal, and tensile properties of produced films were

evaluated. The results showed that the thickness, moisture content, and water

solubility increased with the addition of plasticizer concentration. Regardless of

plasticizer sort, the tensile stress and modulus of plasticized films decreased as the

plasticizer concentrations were raised beyond 25%. Likewise, the relative crystallinity

decreased by increasing the plasticizer content from 0% to 25%, but it began to grow

once the concentration increased above 25%. The fructose-plasticized films presented

consistent and more coherent surfaces compared to sorbitol and urea counterparts. In

summary, the plasticizer types and concentrations are significantly affected on the

performance of the cornstarch-based film, especially for 25% fructose addition.

In the third stage, biodegradable composite films were prepared by using different

concentrations of husk fiber as a reinforcing filler to the optimum biopolymer

produced from the previous stage. The findings indicated that the incorporation of

husk fiber, in general, enhanced the performance of the composite films. There was a

noticeable reduction in the density, moisture content of the films, and soil burial

assessment showed less resistance to biodegradation. The morphological images

presented a consistent structure and excellent compatibility between matrix and

reinforcement, which reflected on the improved tensile strength and modulus as well

as the crystallinity index.

In the last stage, hybrid composites were successfully prepared by loading different

concentrations of sugar palm fiber to the best composite from the previous stage. The

incorporation of sugar palm fiber increased the thickness and the crystallinity index

while reducing the density, moisture content, water solubility, water absorption, and

water vapor permeability of the films. The tensile strength and modulus of the films

were increased from 6.8 MPa to 19.05 MPa and from 61.15 MPa to 1133.47 MPa

respectively for the film contains 6% sugar palm fiber, making it the most efficient

reinforcing.

To sum up, corn husk/sugar palm fiber reinforced cornstarch hybrid composite films

as anticipated, improved the mechanical properties, and the water barrier

characteristics. Thus, they are suitable for replacing conventional non-biodegradable

materials in many applications.

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Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai

memenuhi keperluan untuk ijazah Doktor Falsafah

PENCIRIAN SERAT JAGUNG/ENAU DIPERKUKUHKAN BERSAMA

KANJI JAGUNG BIOPOLYMER HIBRID KOMPOSIT

Oleh


Disember 2019

Pengerusi

Fakulti

: Profesor Ir. Mohd Sapuan bin Salit, PhD, PEng

: Kejuruteraan

Kebimbangan terhadap alam sekitar, seperti bahan pelupusan tidak biodegredasi dan

pembuangan sampah sarap yang semakin meningkat telah memberi ancaman kepada

ekologi. Ruang pelupusan sampah adalah terhad dan kapasiti kawasan pembakaran

tambahan memerlukan pelaburan modal yang tinggi, telah menyebabkan masalah

persekitaran yang berleluasa. Semua isu ini telah memaksa para penyelidik dan saintis

untuk bergerak ke arah pembangunan bahan-bahan mesra alam daripada sumber yang

boleh diperbaharui untuk menggantikan bahan konvensional yang tidak boleh

dibiodegredasi. Diantara sumber-sumber ini adalah tumbuhan jagung dan pokok enau

yang merupakan sumber yang penting bagi kebanyakkan biomas. Oleh itu, satu siri

eksperimen makmal melalui teknik pengacuan cairan telah dijalankan untuk

menyediakan sampel. Seterusnya pencirian kanji, serat, polimer, komposit dan

komposit hibrid dalam empat peringkat turut dijalankan untuk mencapai komposit

hibrid daripada serat jagung/enau diperkukuhkan kanji jagung.

Peringkat pertama direka untuk mengkaji komposisi kimia, sifat fizikal, kestabilan

termal, dan morfologi permukaan termoplastik kanji jagung, sekam jagung, dan

tangkai jagung, yang diekstrak daripada pelbagai bahagian pokok jagung. Sampel

yang diperoleh telah diasingkan dalm bentuk serbuk. Sekam jagung dan kanji jagung

menunjukkan kombinasi ciri-ciri yang terbaik. Sekam jagung mengandungi

kandungan selulosa yang tertinggi (45.7%) serta permukaan morfologi yang

memuaskan. Kanji jagung menunjukkan kandungan amilosa yang baik (24.6g/100g)

dan kestabilan terma yang mampu boleh diterima dengan titik lebur permulaan

sebanyak 161.2 ºC. Fungsi dan struktur biomolekul diantara selulosa dan kanji

menunjukkan hubungan yang sangat baik. Oleh itu, kedua-dua kanji dan sekam jagung

mempunyai potensi untuk digunakan dalam banyak aplikasi biomaterial.

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Tahap kedua telah dicapai bagi menyelidik kesan pelbagai ukuran kepekatan

plasticizer terpilih dalam filem berasaskan kanji jagung dan juga untuk menyediakan

biopolimer baru. Ciri-ciri fizikal, morfologi, haba, dan ketegangan filem yang

dihasilkan telah dinilai. Keputusan menunjukkan bahawa ketebalan, kandungan

kelembapan, dan kelarutan air meningkat dengan penambahan kuantiti plasticizer.

Berbeza dengan jenis plasticizer, tekanan tegangan dan modulus filem plastik semakin

berkurang apabila kandungan plasticizer meningkat melebihi 25%. Begitu juga,

kekristalan relatif mulai menurun dengan meningkatkan kandungan plasticizer dari

0% hingga 25%, namun ianya mula meningkat apabila kandungan plasticizer

meningkat melebihi dari 25%. Filem fructose-plasticized menemukan permukaan

yang konsisten dan lebih koheren berbanding dengan tindak balas sorbitol dan

bahagian urea. Akhirnya, jenis plasticizer dan kandungan kepekatan akan terjejas

dengan ketara terhadap prestasi filem berasaskan cornstarch, terutamanya untuk

penambahan fruktosa 25%.

Pada peringkat ketiga, filem komposit biodegredasi disediakan dengan menggunakan

kandungan kepekatan serat sekam yang berbeza untuk pengukuhan biopolimer secara

optimum yang dihasilkan dari peringkat yang sebelumnya. Penemuan menunjukkan

bahawa penggabungan gentian sekam, secara amnya, meningkatkan prestasi filem

komposit. Terdapat pengurangan yang ketara dalam ketumpatan, kandungan

lembapan filem, dan penilaian pengebumian tanah menunjukkan rintangan yang

berkurangan terhadap biodegradasi. Imej morfologi membentangkan struktur yang

konsisten dan keserasian yang sangat baik antara matriks dan penguat, yang

mencerminkan peningkatan kekuatan tegangan dan modulus serta indeks kritalisasi

yang lebih baik.

Pada peringkat yang terakhir, komposit hibrid telah berjaya disediakan dengan

memuatkan kandungan serat enau yang berbeza ke komposit yang terbaik berbanding

eksperimen terdahulu. Penggabungan serat enau meningkatkan ketebalan dan indeks

kristaliniti. Disamping itu, ia juga sambil mengurangkan kepadatan, kandungan

kelembapan, kelarutan air, penyerapan air dan kebolehterapan wap air dari filem.

Kekuatan tegangan dan modulus filem meningkat dari 6.8 MPa ke 19.05 MPa dan dari

61.15 MPa menjadi 1133.47 MPa bagi filem ini mengandungi 6% serat enau,

menjadikannya cara pengukuhan yang paling berkesan.

Kesimpulannya, serat enau/jagung diperkukuhkan bersama kanji jagung hibrid

komposit film meningkatkan sifat mekanikal dan sifat menghalang air. Oleh itu, bahan

ini sesuai untuk menggantikan bahan konvensional tanpa biodegredasi dalam pelbagai

jenis aplikasi.

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ACKNOWLEDGEMENTS

بسم الله الرحمن الرحيم

In the name of Allah, the Most Gracious, the Most Merciful

Foremost, the highest gratitude to Allah SWT for granting me the strength, resilient,

and knowledge to complete this thesis. The accomplishment of this thesis would not

have achieved without His blessing and guidance. My most profound appreciation

goes to my honorable supervisor Professor Ir. Dr. Mohd. Sapuan Salit for his massive

support and enthusiastic supervision throughout my Ph.D. program. Besides that, I

would like to express my sincere appreciation for the guidance and coaching of my

co-supervisors, Associate Professor Dr. Edi Syams Zainudin (Department of

Mechanical and Manufacturing Engineering, UPM) and Dr. Mohd Zuhri Mohamed

Yusoff (Department of Mechanical and Manufacturing Engineering, UPM) as well as

Dr. Ahmed Edhirej (Department of Chemical and Material Engineering, Sabha,

University, Libya).

I would like to convey my great appreciation to Universiti Putra Malaysia for the

financial support provided through the Universiti Putra Malaysia Grant scheme Hi-

COE.

I owe a special thanks to my beloved father (Ibrahim Jaber) and mother (Madina

Alamin) for the motivations and continuous prayer for my success in this world and

the hereafter. To my dear wife, for her continuous support and sacrifice throughout

my study. Thanks to my siblings, for their constant moral support. It is my fortune to

cheerfully acknowledge the support of my entire family members, including my in-

laws as well as cousins and friends.

My sincere thanks also go to all staff in the Faculty of Engineering and Institute of

Tropical and Forestry Product (INTROP) for their help and guidance. Last but not

least, my thanks go to all those people who knowingly or unknowingly helped me in

the successful completion of this work such as the likes of Dr. Abdoulhdi Amhmad

Borhana Omran (Libyan), and Dr. Ahmed Ilyas bin Rushdan (Malaysian) and many

others.

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This thesis was submitted to the Senate of the Universiti Putra Malaysia and has been

accepted as fulfillment of the requirement for the degree of Doctor of Philosophy. The

members of the Supervisory Committee were as follows:

Mohd Sapuan bin Salit, PhD

Professor, Ir

Faculty of Engineering

Universiti Putra Malaysia

(Chairman)

Edi Syams bin Zainudin, PhD

Associate Professor



(Member)

Mohd Zuhri Mohamed Yusoff, PhD

Senior Lecturer



(Member)

Ahmed Faraj Hissen Edhirej, PhD

Senior Lecturer



(Member)

ZALILAH MOHD SHARIFF, PhD

Professor and Deputy Dean

School of Graduate Studies


Date: © C

OPYRIGHT U

PM

viii

Declaration by graduate student

I hereby confirm that:

this thesis is my original work;

quotations, illustrations, and citations have been duly referenced;

this thesis has not been submitted previously or concurrently for any other degree

at any institutions;

intellectual property from the thesis and copyright of thesis are fully-owned by

Universiti Putra Malaysia, as according to the Universiti Putra Malaysia

(Research) Rules 2012;

written permission must be obtained from supervisor, and the office of Deputy

Vice-Chancellor (Research and innovation) before thesis is published (in the form

of written, printed or in electronic form) including books, journals, modules,

proceedings, popular writings, seminar papers, manuscripts, posters, reports,

lecture notes, learning modules or any other materials as stated in the Universiti

Putra Malaysia (Research) Rules 2012;

there is no plagiarism or data falsification/fabrication in the thesis, and scholarly

integrity is upheld as according to the Universiti Putra Malaysia (Graduate

Studies) Rules 2003 (Revision 2012-2013) and the Universiti Putra Malaysia

(Research) Rules 2012. The thesis has undergone plagiarism detection software

Signature: Date:

Name and Matric No: Mohamed Ibrahim J Ibrahim, GS50780

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Declaration by Members of Supervisory Committee

This is to confirm that:

the research conducted and the writing of this thesis was under our supervision;

supervision responsibilities as stated in the Universiti Putra Malaysia (Graduate

Studies) Rules 2003 (Revision 2012-2013), were adhered to.

Signature:

Name of Chairman

of Supervisory

Committee:

Professor Ir. Dr. Mohd Sapuan Bin Salit

Signature:

Name of Member

of Supervisory

Committee:

Associate Professor Dr. Edi Syams Bin Zainudin

Signature:

Name of Member

of Supervisory

Committee:

Dr. Mohd Zuhri Mohamed Yusoff

Signature:

Name of Member

of Supervisory

Committee:

Dr. Ahmed Faraj Hissen Edhirej

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TABLE OF CONTENTS

Page

ABSTRACT i

ABSTRAK iii

ACKNOWLEDGEMENTS v

APPROVAL vi

DECLARATION viii

LIST OF TABLES xv

LIST OF FIGURES xvii

LIST OF ABBREVIATIONS AND SYMBOLS xix

CHAPTER

1 INTRODUCTION 1 1.1 Background 1 1.2 Problem statements 4 1.3 Research objectives 5 1.4 Significance of study 5 1.5 Scope and limitation of study 6 1.6 Structure of thesis 6

2 LITERATURE REVIEW 8 2.1 Introduction 8 2.2 Corn plant 9

2.2.1 History of corn plant 9 2.2.2 Bioethanol from corn 11

2.3 Corn starch (CS) 12 2.3.1 Corn starch isolation 13 2.3.2 Corn starch film preparation 14 2.3.3 Corn starch properties 14

2.3.3.1 Physicochemical properties 14 2.3.3.2 Pasting properties 16 2.3.3.3 Morphological properties 17 2.3.3.4 Retrogradation properties 18 2.3.3.5 Rheological properties 19

2.3.3.6 Thermal properties (gelatinization) 20 2.4 Corn fibers 20

2.4.1 Cornhusk fiber 20 2.4.2 Cornstalk fiber 21 2.4.3 Corn hull fiber 22

2.4.4 Treatment of corn fiber composites 22 2.4.5 Applications of corn fiber composites 24

2.5 Sugar palm plant 25 2.5.1 History of sugar palm 25 2.5.2 Sugar palm fiber (SPF) 26

2.5.3 Sugar palm fiber composites and applications 27 2.6 Summary 28

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3 MATERIALS AND METHODS 29

3.1 Introduction 29 3.2 Extraction methods of corn biomass 30

3.2.1 Starch extraction 30 3.2.2 Hull fiber extraction 30 3.2.3 Husk fiber extraction 30 3.2.4 Stalk fiber extraction 30

3.3 Preparation of cornstarch-based films 31 3.4 Characterization methods 32

3.4.1 Chemical composition 32 3.4.2 Physical properties 32

3.4.2.1 Particle size distribution (PSD) 32 3.4.2.2 Density and thickness 33 3.4.2.3 Moisture content (MC) 34

3.4.2.4 Water holding capacity (WHC) 34 3.4.2.5 Water solubility (WS) 35 3.4.2.6 Water vapor permeability (WVP) 35 3.4.2.7 Biodegradability test 36

3.4.3 Thermal properties 36 3.4.3.1 Differential scanning calorimetry (DSC) 36 3.4.3.2 Thermal gravimetric analyzer (TGA) 37

3.4.4 Morphological and structural properties 38 3.4.4.1 Scanning electron microscopy (SEM) 38 3.4.4.2 Fourier transform infrared spectroscopy

(FTIR) 38 3.4.4.3 X-ray diffraction (XRD) 39

3.4.5 Tensile properties of films 40

4 EXTRACTION, CHEMICAL COMPOSITION, AND

CHARACTERIZATION OF THE POTENTIAL

LIGNOCELLULOSIC BIOMASSES AND POLYMERS FROM

CORN PLANT PARTS 42 4.1 Introduction 42 4.2 Experimental Details 43

4.2.1 Materials 43 4.2.2 Starch and fibers extraction processes 43 4.2.3 Chemical composition 45

4.2.4 Physical properties 45 4.2.4.1 Density (ρ) 45 4.2.4.2 Moisture content (MC) 45 4.2.4.3 Water holding capacity (WHC) 45 4.2.4.4 Particle size distribution (PSD) 46

4.2.5 Thermal gravity analyzer (TGA) 46 4.2.6 Morphological and structural properties 46

4.2.6.1 Scanning electron microscopy (SEM) 46 4.2.6.2 Fourier transform infrared spectroscopy

(FT-IR) 46

4.2.6.3 X-ray diffraction (XRD) 47 4.3 Results And Discussion 47

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4.3.1 Chemical composition 47

4.3.2 Density and moisture content 48 4.3.3 Water-holding capacity (WHC) 49 4.3.4 Particle size distribution (PSD) 49 4.3.5 Thermal gravity analyzer (TGA) 50 4.3.6 Scanning electron microscopy (SEM) 52 4.3.7 Fourier transform infrared spectroscopy (FT-IR) 53 4.3.8 X-ray diffraction (XRD) 55

4.4 Conclusion 56

5 PHYSICAL, THERMAL, MORPHOLOGICAL, AND

TENSILE PROPERTIES OF CORN STARCH-BASED FILMS

AS AFFECTED BY DIFFERENT PLASTICIZERS 58 5.1 Introduction 58

5.2 Materials and methods 59 5.2.1 Materials 59 5.2.2 Preparation of films 60 5.2.3 Characterization 60

5.2.3.1 Films thickness and density 60 5.2.3.2 Film moisture content (MC) 61 5.2.3.3 Film water solubility (WS) 61 5.2.3.4 Thermal gravimetric analyzer (TGA) 61 5.2.3.5 Scanning electron microscopy (SEM) 61 5.2.3.6 Fourier transform infrared spectroscopy

(FTIR) 62 5.2.3.7 X-ray diffraction (XRD) 62 5.2.3.8 Tensile properties 62 5.2.3.9 Statistical analyses 62

5.3 Results and discussion 62 5.3.1 Thickness and density 62 5.3.2 Moisture content and water solubility 63 5.3.3 Thermal gravimetric analyzer (TGA) 64 5.3.4 Scanning electron microscopy (SEM) 67 5.3.5 Fourier transform infrared (FT-IR) spectroscopy 68 5.3.6 X-ray diffraction (XRD) 71 5.3.7 Mechanical properties 73

5.4 Conclusion 76

6 POTENTIAL OF USING MULTISCALE CORN HUSK FIBER

AS REINFORCING FILLER IN CORNSTARCH-BASED

BIOCOMPOSITES 78 6.1 Introduction 78

6.2 Materials and Methods 80 6.2.1 Materials 80

6.2.2 Composite Films Preparation 80 6.2.3 Thickness and density 81 6.2.4 Moisture Content (MC) 81 6.2.5 Water Solubility (WS) 81 6.2.6 Water Absorption (WA) 82

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6.2.7 Soil Burial Test 82

6.2.8 Scanning Electron Microscopy (SEM) 82 6.2.9 X-ray Diffraction (XRD) 82 6.2.10 Fourier Transform Infrared Spectroscopy (FTIR) 83 6.2.11 Thermal Gravimetric Analysis (TGA) 83 6.2.12 Tensile Properties 83 6.2.13 Statistical analyses 83

6.3 Results And Discussion 83 6.3.1 Thickness and Density 83 6.3.2 Moisture Content 84 6.3.3 Water Solubility 84 6.3.4 Water Absorption 84 6.3.5 Biodegradation of biocomposites 85 6.3.6 Morphological properties 86

6.3.7 X-ray Diffraction (XRD) 87 6.3.8 Fourier Transform Infrared Spectroscopy (FTIR) 88 6.3.9 Thermal Stability 90 6.3.10 Tensile Properties 92

6.4 Conclusion 94

7 PREPARATION AND CHARACTERIZATION OF

CORNHUSK/SUGAR PALM FIBER REINFORCED

CORNSTARCH-BASED HYBRID COMPOSITES 96 7.1 Introduction 96 7.2 Materials and methodology 99

7.2.1 Materials 99 7.2.2 Samples preparation 99 7.2.3 Density (ρ) 100

7.2.4 Moisture content (MC) 100 7.2.5 Water solubility (WS) 100 7.2.6 Water absorption (WA) 101

7.2.7 Scanning electron microscope (SEM) 101 7.2.8 Fourier transform infrared spectroscopy (FTIR) 101

7.2.9 X-ray diffraction (XRD) 101 7.2.10 Thermogravimetric analysis (TGA) 102

7.2.11 Tensile testing 102 7.2.12 Water vapor permeability (WVP) 102

7.3 Results and discussion 103 7.3.1 Density 103 7.3.2 Moisture content 103

7.3.3 Water solubility 104 7.3.4 Water absorption 104

7.3.5 Morphological properties 104 7.3.6 FT-IR analysis 106 7.3.7 Diffraction analysis 107

7.3.8 Thermal properties 108 7.3.9 Tensile properties 110 7.3.10 Water barrier properties 112

7.4 Conclusion 113

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8 CONCLUSIONS AND RECOMMENDATIONS FOR FUTURE

RESEARCH 115 8.1 Conclusions 115 8.2 Recommendations for Future Research 118

REFERENCES 119 APPENDICES 143 BIODATA OF STUDENT 147 LIST OF PUBLICATIONS 148

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LIST OF TABLES

Table Page

2.1 Corn grain composition 11

2.2 World 2015 starch and raw material production 12

2.3 Minor ingredient of maize starch from different references 13

2.4 Different methods of starch isolation 14

2.5 Properties of corn starch 19

2.6 Rheological properties for different corn starch types 20

2.7 Thermal properties of corn starch 20

2.8 Tensile properties of cornhusk fibers 21

2.9 Chemical composition of corn stalk fibers 22

2.10 Methods of fiber treatment 23

2.11 Some products from corn fibers 25

2.12 Chemical composition and mechanical performance of fibers derived

from a variety of sugar palm tree parts 27

4.1 Chemical composition and physical properties of corn starch 47

4.2 Comparison of physicochemical properties of corn fibers with

selected natural fibers 48

4.3 Thermal degradation of corn starch, hull, husk, and stalk 52

5.1 Physical properties of CS-films incorporated with various plasticizers

type and concentration 63

5.2 Degradation temperatures and percentage of residue of CS-films

incorporated with various plasticizers type and concentration 67

5.3 Crystallinity index of CS-films incorporated with various plasticizers

type and concentration 73

6.1 Physical properties of composite films 84

6.2 Crystallinity index of CS/CHF composite films 88

6.3 Degradation temperatures of CS/CHF composites 91

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7.1 Chemical composition and physical properties of corn husk and sugar

palm fibers 99

7.2 Composition of the films at different stages of SPF loading 100

7.3 Physical properties of the films 103

7.4 Crystallinity index of CS-CH/SPF hybrid composite films 107

7.5 Degradation temperatures of CS-CH/SPF hybrid composites 109

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LIST OF FIGURES

Figure Page

2.1 Corn plant parts 10

2.2 Effect of storage on turbidity of corn starch 16

2.3 Pasting properties of different starch sources 17

2.4 Shape of corn starch granule 18

2.5 A typical stress-strain curve of corn husk fibers 21

2.6 Sugar palm tree and sugar palm fiber 26

3.1 Flow processes of methodology 29

3.2 Particle size distribution analyzer 33

3.3 Gas pycnometer 33

3.4 Electronic caliper 34

3.5 Differential scanning calorimeter 37

3.6 Thermal gravimetric analyzer 37

3.7 Scanning electron microscopy 38

3.8 Fourier transform infrared spectroscopy 39

3.9 X-ray diffractometer 40

3.10 Tensile machine 5kN INSTRON 41

4.1 Extraction and preparation of corn biomass 44

4.2 PSD of a) corn starch, b) corn hull, c) corn husk, and d) corn stalk 50

4.3 a) TGA and b) DTG of corn starch, hull, husk, and stalk 51

4.4 SEM of a) corn starch, b) hull, c) husk, and d) stalk 53

4.5 FT-IR spectroscopy of corn starch, hull, husk, and stalk 54

4.6 X-ray diffractogram of corn starch, hull, husk, and stalk 55

5.1 TGA & DTG curves of CS-plasticized films with various plasticizers

type and concentration. (a,b) fructose, (c,d) sorbitol, and (e,f) urea 66

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5.2 SEM images of CS-films with various plasticizers type and

concentration 68

5.3 FTIR curves of CS-films with various plasticizers type and

concentration: (a) fructose, (b) sorbitol, and (c) urea 70

5.4 XRD of CS-films with various plasticizers type and concentration:

(a) fructose, (b) sorbitol, and (c) urea 72

5.5 Tensile properties of CS-films with various plasticizers type and

concentration: (a) Tensile strength, (b) Tensile modulus, and (c)

Elongation at break 75

6.1 Weight loss of CS/CHF composites after soil burial for 20 days 86

6.2 Scanning electron micrograph of CS/CHF composite films with

various CHF concentration 87

6.3 XRD of CS/CHF composite films with various CHF concentration 88

6.4 FTIR curves of CS/CHF composite films with various CHF

concentration 89

6.5 Thermal analysis of CS/CHF composite films. (a) TGA, and (b)

DTG 91

6.6 Tensile properties of CS composite films: (a) Tensile strength, (b)

Tensile modulus, and (c) Elongation at break 93

7.1 Scanning electron micrograph of CS-CH/SPS hybrid composite 105

7.2 FTIR curves of CS-CH/SPF hybrid composites with various SPF

concentration 106

7.3 XRD pattern of CS-CH/SPF hybrid composite with various SPF

concentration 107

7.4 Thermal analysis of CSCH/SPF hybrid composite. (a) TGA, and (b)

DTG 109

7.5 Tensile properties of CS composite films. (a) Tensile strength, (b)

Tensile modulus, and (c) Elongation at break 111

7.6 Water barrier properties of CS-CH/SPF hybrid composites with

various SPF concentration 112

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LIST OF ABBREVIATIONS AND SYMBOLS

Aa Amorphous area

Ac Crystallinity area

CHF Cornhusk fiber

Ci Crystallinity index

CS Corn starch

CSF Cornstalk fiber

DTG Derivative thermogravimetric

Dn Number mean diameter

Dv Number mean volume

FTIR Fourier transform infrared

EB Elongation at break

Minitial Initial mass

Mfinal Final mass

KBr Potassium Bromide

MC Moisture content

PLA Polylactic acid

SEM Scanning electron microscope

SPF Sugar palm fiber

Tc Conclusion temperature

To Onset Temperature

Tp Peak gelatinization temperature

TGA Thermal-gravimetric analysis

TPS Thermoplastic starch

TS Tensile strength

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WA Water absorption

WC Water content

WHC Water holding capacity

winitial Initial weight

wfinal Final weight

WS Water solubility

w/w Weight to weight

WVP Water vapor permeability

XRD X-ray diffraction

di Particle (i) diameter

G’’ Loss modulus

G’ Storage modulus

TG’ Storage modulus temperature

tan ƍ Loss factor

ΔH Enthalpy of gelatinization

ρ Density

θ Diffraction angle

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CHAPTER 1

1 INTRODUCTION

1.1 Background

The accumulation of agricultural residues, together with petroleum-based plastic

wastes, have contributed dramatically to increase environmental pollution to the point

where it has caused problems for natural life and human health as well. The invention

of plastics brought about a revolution in materials production in various sectors such

as the medical, automotive, electronics, packaging, among others (Sharuddin, Abnisa,

Daud, & Arou, 2016). It is characterized by durability, heat resistance, and suitability

for mass production. The global production of synthetic plastics reached 140 million

tons annually, an increase of 2% per year (Shimao, 2001); This indicates that the

percentage of plastic trash that ended up in the landfill is very high and occupies a

large area. Since plastics are clearly valuable and necessary in our daily lives, some

material engineers are trying to develop safer and more environmentally friendly

plastics. Some innovators are developing bioplastics, made from plant crops rather

than fossil fuels, to create more environmentally friendly materials than conventional

synthetic plastics. Others are attempting to fabricate truly biodegradable plastics.

Some researchers are looking for ways to make recycling more effective and hope to

master the process of converting plastics back into fossil fuels from which they are

originated. All these scientists realize that plastics are not perfect but a necessary and

crucial part of our present and future (Pfaendner, 2006). In order to mitigate the issue

of non-biodegradable plastics and biomass waste disposal, the production of

environmentally friendly materials to compensate for long-lasting plastics is inevitable

(Edhirej, Sapuan, Jawaid, & Zahari, 2017d). The development of eco-friendly

materials from natural renewable sources has reduced dependence on conventional

plastics, which in turn contributes to solving the complications of environmental

pollution. In recent times, there has been growing interest in using raw materials and

agricultural by-products in achieving biodegradable plastics, such as from cassava,

potato tubers, sugar palm, and corn. Despite their multi characteristics such as

availability, biodegradation, affordability, and recycling, it is known that bioplastics

developed from natural sources have certain disadvantages, especially in terms of

mechanical performance and water sensitivity compared to fossil sources plastics

(Averous & Boquillon, 2004). Therefore, it is necessary to maintain and increase

research efforts in this area, taking into account the use of local raw materials obtained

from the region such as corn plant, which are studied in research projects, through

which the methodology aims to produce biodegradable plastics can be reproduced on

an industrial scale, taking into account the specific functional requirements of various

applications.

Corn (maize) is a cereal plant belonging to the grass family and is extensively used as

human food, livestock feed, a source of biofuels as well as a raw material in

manufacturing sectors. It was first cultivated in Mexico by local peoples about 10,000

years ago, currently, it is widely cultivated in Latin America, Asia, tropical Africa,

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and North America and it is the most important crop in developing countries, with an

approximate production of 1.4 billion tons in 2014, equivalent to 30% of world’s

grains production (R. Singh, Ram, & Srivastava, 2016). Furthermore, corn is the main

source of commercial starch available, each corn granule (kernel) consists of more

than 70% starch type alpha-linked glucose, and the rest is minor ingredients such as

crude fats, crude proteins, ash, and minerals (McAloon, Taylor, Yee, Ibsen, & Wooley,

2000a). Genetically modified corn starch is widely used as an enhanced matrix for

composites, due to its attractive characteristics such as natural availability,

biodegradability, and affordability. Corn starch applications extend to health check

instruments, electrical appliances, packaging, furniture, and alternative to plastic parts

of automobiles (Guimarães, Wypych, Saul, Ramos, & Satyanarayana, 2010). The

value of harvested corn plant could be improved by obtaining lignocellulosic fibers

from the corn stover (leaves, stems, hulls, and cop). Corn stover typically contains

15% husk, 35% cobs, and 50% stalk; the majority of the stover is discarded as residues

despite their high potential for use as biomass (Sokhansanj, Turhollow, Cushman, &

Cundiff, 2002).

In modern biomaterials science, natural lignocellulosic fibers (NLF) are known to be

unique reinforcing fillers for polymers and composites. Compared to synthetic fillers,

the NLF characterized by many advantages such wide variety and availability,

renewability nature, low density, biodegradability, cost-effective, lower energy

consumption as well as high specific strength and recyclability (Bodirlau, Teaca, &

Spiridon, 2013; Gilfillan, Nguyen, Sopade, & Doherty, 2012). Moreover, it provides

high sound attenuation and relatively easy processing and handling due to its good

flexibility and anti-rust nature that allows high reinforcing quantities (Al-Oqla &

Sapuan, 2014). Natural plant fibers can be obtained from the processing of agricultural

residues. These residues include process residues and field residues; Process residues

are obtained following the crop being processed into valuable resources, includes

seeds, husks, bagasse, molasses, and roots. While field residues indicated to the wastes

left in the cultivation field after harvesting, this type includes leaves, stalks, seeds,

stems, and pods. Both types provide additional value for natural materials (Richards,

Wafter, & Muck, 1984).

Thermoplastic starches (TPS) are natural polymers recognized as one of the promising

biomaterials in the field of biomass production due to their attractive properties that

are combining the affordability, availability, and performance (Abdillahi, Chabrat,

Rouilly, & Rigal, 2013). Therefore, they have been used extensively as a supporting

matrix for the production of bioplastics. However, TPS-based materials revealed

certain drawbacks due to its high hydrophilic characters such as brittleness, water

propensity, and inadequate strength (Averous & Boquillon, 2004). Thus, the

incorporation of enhancing substances like plasticizer is required to alleviate such

drawbacks. The primary function of the plasticizers is reducing the strong attraction

of hydrogen bonds within the starch network and facilitate the mobility of the polymer

particles; this, in turn, improves the flexibility and stiffness of starch-based plasticized

materials (Sanyang, Sapuan, Jawaid, Ishak, & Sahari, 2015). Examples of using

plasticizers as enhancing agents within the starch-based biopolymers have been stated

elsewhere in this thesis. The results indicated that the achieved TPS plastic polymers

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still had insufficient dimensional stability and proved more brittleness as they lost

water or were exposed to high humidity. These shortcomings are severely restricted

to their wide application.

Due to the high correlation between the starch polymer and cellulose fiber, many

material researchers have moved towards enhancing the performance of TPS-based

materials by incorporating natural cellulosic fiber as reinforcing fillers to form a

biocompatible composite. Significant improvement was observed in the final product,

particularly in terms of mechanical characteristics and water barrier properties. For

instance, Edhirej et al., (2017b) produced biocomposites films by filling the cassava

TPS matrix with cassava bagasse. Rabe et al., (2019) investigated the influence of

coconut fiber on corn TPS biocomposites. Hassan et al., (2019) reinforced potato TPS

by PLA. Gazonato et al., (2019) studied the thermomechanical properties of the

cornstarch-based film filled with coffee ground waste. Although acceptable properties

have been achieved, the results suggest upgrading the tensile properties and water

barrier characteristics in order to further improve in the performance and extend the

usability.

In an attempt to settle such deficiencies, incorporating two or more different fibers

into a single matrix might be led to the development of hybrid biocomposites with

better characteristics. The behavior of the hybrid material is a weighted sum of an

individual constituent in which there is a more appropriate balance between inherent

advantages and disadvantages, also, using more than a single fiber type, the

advantages of one type of fiber can substitute what the other lacks (Edhirej et al.,

2017a). In general, the characteristics of the hybrid composite depend mainly on the

fiber content, the particle size distribution of the individual fiber, the bonding of the

fibers to the matrix, the arrangement of both fibers as well as the compatibility of the

failure strain of the fibers used (Sreekala, George, Kumaran, & Thomas, 2002). As a

consequence, hybridization with a fiber characterized by high-water resistance such

as sugar palm fiber is expected to provide better results. The sugar palm tree is a

member of the Palmy family (Siregar, 2005). It mostly planted in tropical regions that

cover southeast Asia and north Australia. Also, it is a multi-purpose tree besides being

a potential source of starch and natural fiber (Ishak et al., 2013).

Sugar palm fiber (SPF) is a natural lignocellulosic fiber characterized by high

resistance to seawater, high tensile strength, low degradation rate, and durability

(Ilyas, Sapuan, Ishak, & Zainudin, 2017). The preparation of SPF requires no effort,

as it does not involve any secondary processing or treatment such as mechanical

decorticating or water ratting (Edhirej, Sapuan, Jawaid, & Zahari, 2017a). In the field

of composite materials, many studies have been published about the utilization of

sugar palm fiber as a reinforcing agent with the polymer matrix. The results indicated

that sugar palm fibers have the potential to be used in many applications of composite

materials, especially those requiring high water resistance.

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This study will focus on the manufacturing of a biohybrid composite material by using

agricultural residues (biomass) of corn and sugar palm trees; these hybrid

biocomposites will be used as an alternative to synthetic plastic composites. Therefore,

the objectives of this research are to extract starch and potential fibers from corn plant

parts such as stalk and husk and then develop a biopolymer by adding different

plasticizers then combining corn starch and corn fiber to produce biocomposites.

Finally, eco-friendly and degradable hybrid materials will be produced using corn

starch as matrix and corn/sugar palm fiber as reinforcement. Characterization

processes will be accompanied by preparation procedures in terms of mechanical

performance, thermostability, physical, and morphological properties.

1.2 Problem statements

Annually, millions of tons of residues remain as a by-product of agriculture crops such

as corn, wheat, barley, rice, cassava, sugarcane, etc. Agricultural residues are materials

left on cultivated land after the crop has been harvested, varying greatly in properties

and decomposition rates (Lal, 2005). Globally, it is estimated that between 2003 and

2013, the production of agricultural residues increased by 33 %, reaching 5 billion

tons in 2013. The Asian continent is the largest producer of crop residues, 47 % of the

total, followed by America (29 %) Europe (16 %), Africa (6 %), and Oceania (2 %)

(Cherubin et al., 2018). These residues caused substantial environmental issues, such

as increased CO2 and other greenhouse gas emissions, soil degradation, biodiversity

loss, and water degradation due to excessive nutrient leaching (Foley et al., 2011).

Corn plant is one of the major sources of agriculture residues in the form of stover;

the global production of corn residues reached 1016.7 million tons in 2013. The

production of corn residues in Asia reaching 304.3 million tons, this accounts for

approximately 30 % of the total global production (Cherubin et al., 2018). Corn stover

typically consists of 50% stalk (stem), 35% leaves and cobs, and 15% husk. Most of

the stover is disposed of as waste, while it is likely to be detected as natural fiber

(Sokhansanj et al., 2002). These residues are generally left to compost in the fields or

are incinerated. The incineration of agricultural wastes continually generates a large

amount of greenhouse gases like carbon dioxide, methane, nitrous oxide, and ozone.

Such gasses have a negative impact on health and contribute to global warming and

global pollution as well.

In response to community demand to dispose of agricultural and polymeric wastes that

have environmental problems, finding value-added uses of these undervalued field

crop residues together with bio-based polymers may help maintain a carbon dioxide

balance and has the potential of reducing problems associated with emissions

produced during the manufacturing of petroleum-based composites and from field

waste incineration. Therefore, the preparation and development of environmental

materials derived from sustainable resources are considered an appropriate solution

for waste management and alternative to petroleum-based materials. Such bio-

resources are having a positive impact on air, land, water, and characterized by

renewability, availability, biodegradability, and cost-effective. Natural cellulose fibers

and polymers typically extracted from plant residues have great potential to meet the

requirements of environmental complications. A systematic approach on how to select

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the best biopolymer and natural fiber, along with the best conceptual design, that helps

to reduce the environmental impact of the entire product life cycle. Hence, it is

necessary to maintain and increase the research efforts in the field of composite

biomaterials, taking into account the use of local raw materials sourced in the region

such as corn plant and sugar palm tree, which are being studied in research projects,

through which it is intended that the methodology production of biodegradable plastics

is reproducible on an industrial scale, considering the specific functional requirements

for various applications.

1.3 Research objectives

The research objectives of this study are: -

1. To characterize starch and potential fibers from corn plant parts (hull, husk,

and stalk) in order to prepare and develop a new biodegradable and

environmentally friendly composite.

2. To investigate the physical, mechanical, thermal, and morphological

properties of the cornstarch-base films as affected by different plasticizers.

3. To investigate and characterize the potential of using multiscale corn husk

fiber as reinforcing filler in cornstarch-based biocomposites.

4. To determine and characterize the effect of sugar palm fiber loading on

corn/sugar palm fiber reinforced cornstarch hybrid composites.

1.4 Significance of study

1) Development of a new biodegradable hybrid composite characterized by low

in cost production, renewable, biodegradable, and environmentally friendly

for use in a variety of industrial applications as an alternative to non-

biodegradable petroleum plastics.

2) Substituting petroleum-based polymers with TPS-based polymers may

reduce the growth rate of petroleum polymers, thereby reducing the health

effects resulted from it and reducing dependence on petroleum.

3) The utilization of corn plant and sugar palm residues, which are highly

abundant and inexpensive that may contribute to mitigate the problem of

wastes and responds to the community's demand for agricultural and

polymeric waste disposal, which also improves the economic growth through

the transfer from waste to wealth.

4) Besides, this research provides a cognitive contribution to product design

specifications, material selection analysis, conceptual design development,

and conceptual design selection.

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1.5 Scope and limitation of study

In the current research, cornstarch (CS) and corn hull fiber were derived from fresh

corn ear, while corn husk and stalk fibers were extracted from the leaves and stems of

corn plants, respectively. The obtained biomasses in powder form were characterized

in terms of physical, thermal, structural, morphological properties, and chemical

composition as well. The influence of various plasticizers kind and concentration on

physical, thermal, tensile, and structural properties of cornstarch based-film were

evaluated. The criteria for selection were mainly based on the best physical and tensile

properties. Hence, the CS-plasticized film with optimum characteristics was

reinforced with corn husk fiber CHF (the best fiber) at different loadings (0, 2, 4, 6,

and 8%). The optimal fibrous loading ratio of the obtained composite films was then

selected based on the physical and tensile properties supported by morphological,

structural, and thermal properties. After that, the selected composite film was

hybridized by sugar palm fiber (SPF) at different concentrations (2, 4, 6, and 8% w/w

dry starch). The specimens achieved were tested for their tensile and thermostability

properties along with other analyses such as XRD, FTIR, and SEM. Finally, the CS-

CH/SPF hybrid composites were submitted to the water barrier assay and

biodegradation test to investigate its environmental impact.

It should be noted that all film samples were prepared using the solution casting

technique into an aqueous medium containing distilled water, and all concentrations

of the used substances were calculated based on the weight of corn starch (5g).

Furthermore, there was not any treatment or modifying the chemical structure of the

materials used in the current work.

1.6 Structure of thesis

The outline of the thesis is following the alternative thesis format of Universiti Putra

Malaysia based on publications, in which each research chapter (4-7) represents a

separate study it is own included: 'Introduction,' 'Materials and methods,' 'Results and

discussion,' and 'Conclusion.' The details of the thesis structure are presented below.

Chapter 1

The problem statement and research objectives are clearly described in this chapter.

Furthermore, the importance and contribution of the research, as well as the scope and

limitation of the study, were also illustrated in this chapter.

Chapter 2

A comprehensive review of the literature on the critical areas related to the subject of

this thesis is presented in this chapter.

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Chapter 3

This chapter of the methodology includes every activity related to this research, from

the beginning of material preparation to material processing, testing procedures, and

data collection and analysis.

Chapter 4

This chapter presents the first article entitled “Extraction, Chemical Composition, and

Characterization of Potential Lignocellulosic Biomasses and Polymers from Corn

Plant Parts.” In this article, the physical, morphological, structural, and thermal

properties of a cornstarch and corn hull, husk, and stalk fibers were evaluated.

Chapter 5

This chapter presents the second article entitled “Physical, Thermal, Morphological,

and Tensile Properties of Cornstarch-Based Films as Affected by Different

Plasticizers.” In this article, the influence of different plasticizer types (fructose,

sorbitol, and urea) at concentrations (25, 40, and 55%) on the properties of the corn-

based film was investigated.

Chapter 6

This chapter presents the third article entitled “Potential of Using Multiscale Corn

Husk Fiber as Reinforcing Filler in Cornstarch-Based Biocomposites” This article

focused on producing and characterizing of biocomposite films based on cornstarch

matrix and cornhusk fiber as reinforcement filler at different loadings.

Chapter 7

This chapter presents the fourth article entitled “Processing and Characterization of

Corn/Sugar Palm Fiber Reinforced Corn Starch Biopolymer Hybrid Composites.”

This article studied the effect of various loading of sugar palm fiber (2%, 4%, 6%, and

8%) on the physical, thermal, structural, tensile, and water barrier properties of

thermoplastic cornstarch-based hybrid composite contains 25% of fructose plasticizer

and 8% of cornhusk fiber.

Chapter 8

This chapter provides general conclusions from various research articles, as well as

relevant suggestions and recommendations for future research.

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